Method of manufacturing a material that reacts with air in an inert atmosphere

ABSTRACT

Manufacturing a material having at least one metal component which reacts with air in an inert atmosphere comprising sucking said liquid into part of a tube, cooling said tube and liquid in the inert atmosphere to cause the material to solidify and expelling the molded solid material from said tube.

Uni-ted States Patent [72] Inventor [50] FieldofSearch..v.......................................... l64/47,63, 65, 66,131, 253, 259, 344; 18/30 QI-l References Citedl UNITED STATES PATENTS 1/1856 Ripley.......................... 3/1909 Smith Hendricus Elise Michel Cornelus Vos Emmasingel, Eindhoven, Netherlands 805,280

Appl. No. [22) Filed Mar. 7, 1969 Patented Dec. 21, 1971 [73] Assignee U.S. Philips Corporation 14,115

New York, N.Y. 914 679 [32] Priority Mar-19,1968 2,379,401 6/1945 Poulter.

Netherlands 1 FOREIGN PATENTS 11/1965 Canada Primary Examiner-R. Spencer Annear Attorney-Frank R. Trii'ari [54] METHOD OF MANUFACTURING A MATERIAL ABSTRACT: Manufacturing a material having at least one metal component which reacts with air in an inert atmosphere comprising sucking said liquid into part of a tube, cooling said tube and liquid in the inert atmosphere to cause the material to solidify and expelling the molded solid material from said tube.

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INVENTOR.

HENDRICUS EIMC. VOS

BY V

AGENT METHOD OF MANUFACTURING A MATERIAL THAT REACTS WITH AIR IN AN INERT ATMOSPHERE The invention relates to a method of manufacturing in an atmosphere of inert gas grains of a material containing-at least one metal which reacts with air.'A drawback of the known method of the kind described is, for example, that when starting from a liquid state of the material and after isolation of a few portions of this material the liquid substances of these por-' tions flow together. This gives rise to the situation that no grains of constant volume are obtained after solidification of the isolated material. A further possibility is, to pour the liquid starting material into cavities of a plate which is subsequently cooled. The liquid portions then solidify in the cavities, thus making it possible to manufacture lozenges, pills or other granular doses. However, a rather intricate plate is required for the latter method. 7

his an object of the invention to obviate or at least to mitigate the above-mentioned drawbacks.

A method according to the invention for manufacturing in an atmosphere of inert gas grains of a material containing at least one metal which reacts with air is characterized in that a quantity of liquid material contained in a supply vessel is first drawn into a tube provided with a sucker whereafter the part of the tube filled with this material is moved to a rest place at a temperature at which this material solidifies, that subsequently solidification of this material is awaited and that then the solidified material is expelled from the tube into an auxiliary vessel with the aid of the sucker.

An advantage of the method according to the invention is that there is no risk'of isolated liquid doses of the material flowing together. In fact this material is introduced into an auxiliary vessel only after solidification of the isolated material at a rest place. In a method according to the invention an intricate plate having cavities as referred to above is not necessary.

The starting material consists, for example, of one metal which reacts with air, for example, sodium. It is, however, alternatively possible for the material to consist of a mixture or of an alloy. The starting material is, for example, sodium amalgam.

[t is feasible that the sucker and the tube are operated through magnetic forces which act through the wall of a vessel.

A method according to the invention is preferably carried out in such a manner that the sucker and the tube are operated at the end of the tube remote from the supply vessel, this end being exposed to the air. An advantage of this method is that the tube and sucker can be operated in a simple manner either manually or mechanically.

It is feasible that the two vessels (the supply vessel and the auxiliary vessel) can be displaced relative to the tube. For example, after sucking up liquid material from the supply vessel, the tube is pulled upwards, subsequently the supply vessel is displaced and the auxiliary vessel is put underneath the tube, and finally the grain is expelled from the tube into the auxiliary vessel.

A method according to the invention is preferably carried out in such a manner that prior to expelling the solidified material from the tube, this tube is slightly tilted and the solidified material in the tube is introduced into an inlet aperture towards the auxiliary vessel.

An advantage of this preferred method is that the vessels may remain in place. In this case it is only necessary to move the tube. It is feasible that the liquid material is allowed to stand at the rest place until it solidifies of its own accord.

The rest place is preferably cooled by means of a forced cooling, for example, by cooling air. An advantage of the lastmentioned preferred method is that the tube must stand at the rest place for only a short period. This enhances the speed of production.

It is feasible that the two vessels are present in a large inert gas-filled space or cabinet, for example, in a so-called glove box."

The method according to the invention is preferably carried out in a device containing an inert gas in the operating condition which inert gas is only present in a supply vessel and an auxiliary vessel and in a connection between these two vessels.

An advantage of this device is that it may be considerably smaller than in the case of the said glove box." This advantage becomes manifest, inter alia, in that considerably less time is required for starting a preferred device according to the present invention and filling it with an inert gas than in the case of a glove box."

It is of course feasible that the tube is provided with an operating device of the sucker which acts with a screw thread or a different operating mechanism.

The tube of a device according to the invention preferably has at the end remote from the supply vessel, a pushbutton for operating the sucker.

This preferred solution has the advantage that the operation of the sucker is very simple.

It is feasible that the supply vessel has the shape of a cubical container, the tube protruding through an aperture in the upper surface of this container. It is then possible to place the tube in the aperture of the container by means of, for example, a rubber lead-through cylinder in such a manner that the aperture is sealed in a gastight manner. This situation will, for example, occur when in manufacturing a large number of grains, operations are carried out in always the same atmosphere of inert gas.

The supply vessel preferably forms part of a bottle-shaped envelope, in which the tube protrudes through the aperture of this envelope, and the inlet aperture of the auxiliary vessel is provided in the bottle-shaped envelope above the supply vessel.

This device has the advantage that it may be very small and that possible tilting movements of the tube may be reduced to aminimum.

In an advantageous embodiment of a device according to the invention the inlet aperture for gas is provided in the bottle-shaped envelope, namely between the supply vessel and the inlet aperture of the auxiliary vessel, the tube incompletely closing the neck of the bottle-shaped envelope.

An advantage of this preferred solution is that both a small device can be obtained and that new has can be used every time which enters through the inlet aperture for gas and leaves the device again through the incompletely closed neck of the bottle. In fact, this has the advantage that possible pollutions in the device are removed by the gas which is constantly resupplied.

It is possible to suspend the end of the tube remote from the liquid material to a bracket so that the other end of the tube is present at the so-called rest place.

Preferably, however, a support for the tube is provided near the inlet aperture of the auxiliary vessel.

This solution is considerably simpler than, for example, the above-mentioned suspension in the bracket.

In a particularly advantageousembodiment of the device the said support for the tube is formed by an extended wall portion of the auxiliary vessel.

The operation device of the sucker in the tube preferably has a stop.

An advantage thereof is that it is possible to always produce equal grains.

If a device according to the invention is used for manufacturing sodium amalgam grains, the supply vessel is preferably provided with a heating element.

An advantage thereof is that it is not necessary to heat the sodium amalgam (which is solid at room temperature) elsewhere and to subsequently pour it over into a supply vessel.

The sodium amalgam grains produced may, for example, be used in the discharge tube of a high-pressure sodium discharge lamp.

The auxiliary vessel may be a bottle which is sealed in a gastight manner after introduction of the grains. This bottle may then be stored until further use.

It is feasible that the auxiliary vessel forms the future discharge tube of a lamp. An advantage of this solution is that the temporary storage of the grains is completely unnecessary.

In order that the invention may be readily carried into effect, a few embodiments thereof will now be described in detail by way of example with reference to the accompanying diagrammatic drawing, in which:

FIG. 1 shows a device for carrying out a method according to the invention, 7

H0. 2 shows the same device as that is FIG. 1, however, in a different stage of manufacture.

In FIG. 1 a supply vessel is indicated by l, which forms part of a bottle-shaped vessel 2. The supply vessel 1 contains liquid sodium amalgam 3. The supply vessel 1 is partly surrounded by a heating device 4. This device consists of an electrical heating element 5 and a container 6 which is filled with sand 7. The side of the bottle-shaped envelope remote from the heating device 4 has an aperture 8. A tube 9 including a sucker l0 protrudes through the aperture 8. In the situation shown in figure 1 one end of the tube 9 is immersed in the liquid sodium amalgam 3 in the supply vessel 1. A pushbutton 11 connected to the sucker is provided at the other end of the tube 9. This pushbutton forms part of a mechanism 12 which abuts against an end part 13 of the tube 9 when the sucker is pulled upwards. A compression spring 14 is provided between the part 12 of the pushbutton mechanism and an internal part of the tube 9. An auxiliary vessel is indicated by 15. The auxiliary vessel l5 communicates through the aperture 16 with the bottle-shaped vessel 2. The auxiliary vessel is surrounded by a hollow cylinder 17 having an aperture 18 into which cooling air is blown. The side of the cylinder 17 remote from the aperture 18 is also open. As a result the cooling air can flow away again. An extended wall portion of the auxiliary vessel 15 is indicated by 19, while the lead-through aperture for the supply of an inert gas into the vessels is indicated by 20. In a concrete case argon gas is supplied through the aperture 20 (see FIG. 1, double arrow). This gas escapes again at the aperture 8 of the bottle-shaped vessel 2. Grains of sodium amalgam already manufactured are indicated by 21, 21 and 21".

The method which is carried out with the aid of the device described is as follows. First the initially depressed pushbutton I1 is released. Due to the spring action of the spring 14 the sucker 10 in the tube 9 will rise to a certain extent (until portion 12 abuts against 13). As a result amalgam is sucked up from the main vessel 1. Subsequently the tube is pulled upwards, and tilted to a slight extent. This is effected in such a manner that the tube 9 acquires the rest position shown in FIG. 2. In this rest position one end of the tube 9 bears on the extended wall portion 19 of the auxiliary vessel'l5. It is to be noted that corresponding parts of the FIGS. 1 and 2 have the same reference numerals.

In the situation of FIG. 2 the tube 9 is placed in such a manner that its lower end is in a-rest position which is so cool that the isolated amount of liquid sodium amalgam near the sucker in the tube solidified. In a concrete case in which cooling air was introduced through the aperture 18, the said material in the tube had sufficiently solidified after approximately 15 seconds. After solidification, pushbutton 11 is depressed again so that the solidified material is expelled from the tube 9 with the aid of the sucker 10. This solidified material then glides, in the shape of a small cylinder, into the auxiliary vessel 15.

Subsequently the tube 9 is tilted back again and placed again in the supply vessel such that the end of the tube including the sucker I0 is immersed in the sodium amalgam liquid. The procedure described is repeated for the manufacture of subsequent grains. Meanwhile argon gas always flows through the aperture 20 to aperture 8. This gas prevents an attack of the sodium amalgam. The content of the device described was approximately 0.5 liter.

Instead of the cylindrical shape the grains may alternatively acquire different shapes. To this end, however, a different cross section of the tube 9 will have to be chosen.

The present invention 18 in no way limited to the manufacture of sodium amalgam grains, but may for example, alternatively be used for manufacturing grains of different materials of which at least one part consists of metal which reacts with air.

What is claimed is:

1. A method of manufacturing a material consisting essentially of sodium amalgam comprising heating said material in a supply vessel, containing, an atmosphere of inert gas to prevent a reaction of said material with air while maintaining said material in a liquid state, using a sucker to draw a predetermined quantity of said liquid from said supply vessel into an open end of a tube passing through said supply vessel, cooling the open end portion of said tube containing said material in said inert atmosphere to solidify the material, and expelling said solidified material from said tube into an auxiliary vessel having an inert atmosphere.

2. A method of manufacturing as claimed in claim 1 wherein said drawing is operated from the end of said tube exposed to air and remote from the supply vessel.

3. A method of manufacturing as claimed in claim 1 wherein expelling said solidified material from said tube comprises tilting said tube slightly prior to the expulsion and introduction of said solidified material into an inlet aperture of said auxiliary vessel.

4. A method of manufacturing as claimed in claim 1 wherein cooling the open end portion of said tube comprises cooling by means of air.

* i i k 

1. A method of manufacturing a material consisting essentially of sodium amalgam comprising heating said material in a supply vessel, containing, an atmosphere of inert gas to prevent a reaction of said material with air while maintaining said material in a liquid state, using a sucker to draw a predetermined quantity of said liquid from said supply vessel into an open end of a tube passing through said supply vessel, cooling the open end portion of said tube containing said material in said inert atmosphere to solidify the material, and expelling said solidified material from said tube into an auxiliary vessel having an inert atmosphere.
 2. A method of manufacturing as claimed in claim 1 wherein said drawing is operated from the end of said tube exposed to air and remote from the supply vessel.
 3. A method of manufacturing as claimed in claim 1 wherein expelling said solidified material from said tube comprises tilting said tube slightly prior to the expulsion and introduction of said solidified material into an inlet aperture of said auxiliary vessel.
 4. A method of manufacturing as claimed in claim 1 wherein cooling the open end portion of said tube comprises cooling by means of air. 